CN1787125A - Iron-base non-crystal alloy powder, magnetic powder core with excellent high frequency performance and preparation process thereof - Google Patents

Iron-base non-crystal alloy powder, magnetic powder core with excellent high frequency performance and preparation process thereof Download PDF

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CN1787125A
CN1787125A CNA2005101149334A CN200510114933A CN1787125A CN 1787125 A CN1787125 A CN 1787125A CN A2005101149334 A CNA2005101149334 A CN A2005101149334A CN 200510114933 A CN200510114933 A CN 200510114933A CN 1787125 A CN1787125 A CN 1787125A
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amorphous
magnetic core
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alloy
magnetic
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CN100442402C (en
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卢志超
陆曹卫
李德仁
孙克
周少雄
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Advanced Technology and Materials Co Ltd
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Central Iron and Steel Research Institute
Advanced Technology and Materials Co Ltd
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    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
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Abstract

The invention provides an excellent-high frequency performance noncrystalline alloy powder and the magnetic powder core preparing method thereof. And the atomic percentage composition of the alloy powder meets the relationship: (Fe1-xMx)100-a-b-cPaTbDc , where M =at least one of the Co and Ni; T = at least above three of the Al, C, B and Si; D= one or several of the Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, Pd and Au; x=0.01-0.16; a=8-15; b=10-25; c=0.5-6. It mills the alloy powder by pulverization, and prepares the milled powder into the noncrystalline alloy magnetic core powder by screening, insulating, pressing, annealing and paint spraying processes.

Description

Have Fe-based amorphous alloy powder, magnetic core of excellent high frequency performance and preparation method thereof
Technical field
The present invention relates to a kind of Fe-based amorphous alloy powder, particularly about the amorphous powdered alloy of powder soft magnetism, use magnetic core of this powder preparation and preparation method thereof.
Background technology
Fe base amorphous, nano-crystal soft magnetic alloy, for example, the Fe-Si-B that United States Patent (USP) 4217135 provides is the Fe-Cu-M-Si-B that provides of non-crystaline amorphous metal and 4881989 (wherein M is a kind of in the elements such as Nb, Mo, Hf, a Ta) system nano-crystal magnetically soft alloy, owing to have good soft magnet performance, now obtained extensive use as various electronic devices and components.This Fe base noncrystal alloy, the critical cooling rate that needs is very high, is about 10 -5K/s only can pass through single-roller rapid quenching with quenching prepared in batches amorphous band at present, but is difficult to obtain amorphous powdered alloy by direct quick-quenching method.
Fe base amorphous, nanometer crystal alloy powder can pass through the band breaking method is obtained, and its magnetic core can pass through bonding processing, and operations such as compacting, annealing obtain.The problem of this magnetic core is that the powder that breaking method obtains is a flakelike powder, and contains more distortion powder, is difficult to guarantee insulation, and therefore quality factor is lower usually, and loss is higher.
United States Patent (USP) 5,876, the series bulk amorphous system of 519 Fe-Al-Ga-P-C-B-Si that provide, has big amorphous formation ability, its supercooling liquid phase region surpasses 50K, can obtain the above block amorphous alloy of thickness 1.5mm by the method for mold, and this alloy has good soft magnet performance.The Fe base alloy system of this large-amorphous forming capacity can prepare amorphous powdered alloy by atomization method, and powder can be pressed into the magnetic core through bonding processing.The problem of this soft-magnetic alloy powder is, the one, contain Ga, and its price is about 5000 yuan/kilogram, so powder price is high, is difficult to promote; The 2nd, do not contain anti-oxidant elements such as Ni, Cr, antioxygenic property is not good, the easy oxidation of powder during powder by atomization, mis-behave.In addition, Chinese patent CN1487536A provides a kind of Fe base noncrystal alloy system, and this is that alloy contains element P, C, B at least, also contains elements such as a spot of Cr, Mo, W, V, Nb.The constituent content that this alloy system Cr, Mo etc. help improving the powder antioxygenic property is few, and antioxygenic property is not high, makes powder easily oxidation take place when atomizing and performance is not good.
Summary of the invention
One of purpose of the present invention be to provide have concurrently excellent high frequency performance, strong amorphous formation ability, cheaply, the amorphous powdered alloy of low oxygen content that can be by the atomization method preparation and preparation method thereof.
Two of purpose of the present invention be to provide adopt above-mentioned amorphous powdered alloy preparation, have excellent high frequency performance magnetic core and preparation method thereof.
In order to achieve the above object, the present invention is achieved in that
One aspect of the present invention has provided a kind of amorphous powdered alloy with good high-frequency soft magnetic performance, and its alloying component atomic percent composition satisfies relational expression: (Fe 1-xM x) 100-a-b-cP aT bD cWherein, M is at least a among Co, the Ni; T be among Al, C, B, the Si more than three kinds; D be among Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, Pd, the Au at least--plant; X is 0.01-0.16; A is 8-15; B is 10-25; C is 0.5-6.Preferably, x is 0.01-0.12; A is 9-12; B is 10-23; C is 1-5.22≤(a+b+c)≤38。
Reduction glass transformation temperature Trg 〉=0.53 of this amorphous powdered alloy, Trg=Tg/Tm wherein, Tg is a glass transformation temperature, Tm is an alloy melting point.Supercool liquid phase region Δ Tx 〉=20K, Δ Tx=Tx-Tg wherein, Tx is a crystallization temperature.Oxygen content in power is below 4000ppm.
Another aspect of the present invention has provided a kind of preparation method with amorphous powdered alloy of good high-frequency soft magnetic performance, alloy with mentioned component, adopt atomizing type to prepare alloy powder, described atomizing type is water atomization and/or aerosolization, and described aerosol turns to vacuum aerosolization, antivacuum aerosolization, regulate one or more or its combination in the aerosolization.
The apparent density of powder ρ that this method obtains satisfies: ρ 〉=2.4g/cm 3
A third aspect of the present invention has provided a kind of non-crystaline amorphous metal powder magnetic core with good high-frequency soft magnetic performance, comprise following components in weight percentage: insulating compound 0.2%-7%, bonding agent 0.01-5%, lubricant 0.01-2%, all the other are above-mentioned non-crystaline amorphous metal powder.
Wherein, described insulating compound is selected from following at least a or its combination of respectively organizing in the material:
Be selected from SiO 2, Cao, Al 2O 3, TiO 2Oxide powder;
Be selected from the salt of silicates, phosphoric acid salt;
Be selected from mica powder, kaolinic mineral powder; With
The surface film that chemical method generates or the surface oxidation of generation.
Described bonding agent is organic bonding agent and/or inorganic adhesive, wherein: the organic bonding agent be selected from epoxylite, at least a in the epoxylite, inorganic adhesive is selected from least a in the phosphoric acid salt.
Described lubricant is selected from the stearate profit, talcum powder is at least a or its combination.
The magnetic property of this magnetic core satisfy following at least one, several or its combination:
Magnetic permeability is more than 35;
Quality factor q is not less than 30 under 1MHz;
Under 100kHz, be not less than 98% than magnetic permeability, under 1MHz, be not less than 90%;
Maximum field is the pairing coercive force H of the static hysteresis loop of 2000A/m cBelow 70A/m.
A fourth aspect of the present invention has provided a kind of preparation method with non-crystaline amorphous metal powder magnetic core of good high-frequency soft magnetic performance, and this method may further comprise the steps:
(a), adopt insulating compound, bonding agent and the mix lubricant of above-mentioned amorphous powdered alloy and desired content and be dried to dry powder;
(b), above-mentioned dried powder is pressed in makes the magnetic core under the 500MPa-3000MPa pressure;
(c), the magnetic core with press forming carries out annealing in process below the amorphous crystallization temperature.
After described step (c), further may further comprise the steps: (d), the processing of spraying paint of magnetic core; (e), the magnetic core performance detects.
In the described step (c), described magnetic core annealing in process temperature is at (T x-100 ℃) to T xBetween, T xBe the amorphous crystallization temperature; Be annealed into 5 minutes to 300 minutes; Atmosphere is a kind of in vacuum, nitrogen, the argon gas atmosphere.
In the described step (c), annealing temperature is at (T x-70 ℃) to (T x-20 ℃) between, T xBe the amorphous crystallization temperature.
The magnetic property of the magnetic core that this preparation method obtains satisfies following at least one or its combination:
Magnetic permeability is more than 35;
Quality factor q is not less than 30 under 1MHz;
Under 100kHz, be not less than 98% than magnetic permeability, under 1MHz, be not less than 90%;
Maximum field is the pairing coercive force H of the static hysteresis loop of 2000A/m cBelow 70A/m.
In sum, the invention provides a kind of technical scheme for preparing amorphous powdered alloy and amorphous magnetic core thereof, wherein by improvement to alloying component, make antioxygenic property, the amorphous formation ability of alloy be improved, therefore can adopt atomization method prepare amorphous powdered alloy, this powder through insulation processing and with the mixed dry powder that is prepared into of a small amount of bonding agent, compression moulding obtains amorphous magnetic core through appropriate heat treatment.Specifically be described below:
The improvement of alloying component
Amorphous powdered alloy of the present invention is a main component with magnetically soft alloy Fe, contains a spot of Co, Ni, so soft magnet performance is better, and the adding of Co, Ni can improve the antioxygenic property of powder; The present invention simultaneously contains more amorphous forming element P, Al, C, B, Si, therefore can form amorphous powdered alloy; And the present invention can contain more than one in the elements such as Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, Pd, Au, can further improve alloy amorphous formation ability and antioxygenic property.The amorphous formation ability that the adding of element such as Sn, Zr can effectively raising powder for example; And the adding of elements such as Cr, Mo can improve the antioxygenic property of powder when improving amorphous formation ability.
Amorphous powdered alloy of the present invention, its alloying component atomic percent satisfies following formula:
(Fe 1-xM x) 100-a-b-cP aT bD c
Wherein, M is at least a among Co, the Ni; T be among Al, C, B, the Si more than three kinds; D is at least a among Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, Pd, the Au; X is 0.01-0.16; A is 8-15; B is 10-25; C is 0.5-6.
For amorphous powdered alloy of the present invention, Co, the preferred 1at% of Ni content are to 12at%; The preferred 9at% of P content is to 12at%; Al, C, the preferred 10at% of B, Si are to 23at%; Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, the preferred 1at% of Pd, Au are to 5at%.
For amorphous powdered alloy of the present invention, preferred Fe, Co, Ni element sum are that 62at% is to 78at%; Preferred P, Al, C, B, Si, Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, Pd, Au element sum are that 22at% is to 38at%.
Alloy of the present invention can contain a small amount of inevitable 0 and other impurity, and the content sum of other impurity is not more than 0.5wt%.
Atomization prepares amorphous powdered alloy
Amorphous powdered alloy of the present invention has strong amorphous formation ability, can prepare amorphous powdered alloy by atomization method; Its supercooling liquid phase region Δ T x〉=20K (Δ T x=T x-T g, T wherein xExpression crystallization temperature, T gThe expression glass transformation temperature), reduction glass transformation temperature T Rg〉=0.53 (T Rg=T g/ T m, T wherein mThe expression alloy melting point).
Amorphous powdered alloy of the present invention can prepare under antivacuum state by the water atomization method, and its amorphous powdered alloy particle size can reach more than the 75 μ m, and oxygen content in power is below 4000pp.This water atomization amorphous powdered alloy apparent density has following feature: between positive 300 orders (about 49 μ m), apparent density of powder is greater than 2.7g/cm at negative 200 orders (about 74 μ m) for particle size 3To between positive 400 orders (about 38 μ m), apparent density of powder is greater than 2.6g/cm at negative 300 orders (about 49 μ m) for particle size 3Particle size is for below negative 400 orders (about 38 μ m), and more than the 5 μ m, the apparent density of amorphous powdered alloy is greater than 2.5g/cm 3
Among the present invention, preparation magnetic core water atomization amorphous powdered alloy, its oxygen content is that 4000ppm is following.Too high oxygen level, the powder magnetic property worsens; Adopt this powder preparation magnetic core, the magnetic core performance is not good, shows as that magnetic permeability reduces, coercive force is big.
Among the present invention, preparation magnetic core water atomization amorphous powdered alloy, its apparent density is 2.5g/cm 3More than.If apparent density of powder is too little, it is bad to prepare the magnetic core performance.Because apparent density of powder is too small, normally contains reasons such as increased number of stomata in too little or powder shape complexity or the powder and cause owing to particle size.Adopt the magnetic core of this powder preparation, its density is low excessively, and distributed air gaps is too big in the magnetic core, and powder core magnetic permeability is low, and powder core coercive force is big, and loss is higher.Amorphous powdered alloy apparent density of the present invention is 2.5g/cm 3More than, preferred 2.8g/cm 3More than.
It is slow slightly that aerosolization method and water atomization method are compared cooling rate.Alloy system of the present invention, also can pass through vacuum aerosolization, antivacuum aerosolization, adjusting aerosolization (employing gas atomization alloy liquation powdered, the atomization method that adopts water that powder particle is cooled off again) etc. atomization method prepares the amorphous powdered alloy of subglobular, its amorphous powdered alloy particle size can reach more than the 50 μ m, and oxygen content in power is below 1500ppm.The apparent density of aerosolization amorphous powdered alloy is greater than 3.5g/cm 3
Prepare the magnetic core with amorphous powdered alloy
Among the present invention, the used aerosolization amorphous powdered alloy of preparation magnetic core, its oxygen content is that 1500ppm is following.Adopt the magnetic core performance of this powder amorphous powdered alloy preparation good, magnetic permeability height, coercive force are low.Compare with water atomized powder, the magnetic core cost of aerosolization powder preparation increases to some extent, and performance increases, and can satisfy the demand of some high-end products.
The magnetic core method of amorphous powdered alloy preparation of the present invention may further comprise the steps:
1, powder and megohmite insulant, bonding mix and greasing substance mixes and is dried to dry powder;
2, powder compaction becomes the magnetic core;
3, the magnetic core is carried out annealing in process;
4, the magnetic core processing of spraying paint;
5, the magnetic core performance detects.
The amorphous powdered alloy that preparation is finished sieves, and can adopt testing sieve, and standard is bounced realizations such as the reciprocating sieve of formula reciprocating sieve, other types and air-flowing type powder classification equipment.Prepare the magnetic ring according to following steps then:
Step 1
In order to improve magnetic core resistivity, reduce eddy current loss, improve the magnetic permeability under the high frequency, the megohmite insulant of the preferred following kind of the present invention and amorphous powdered alloy carry out mix insulation: 1, oxide powder, as SiO 2, Cao, Al 2O 3, TiO 2Deng, the common stable in properties of oxide powder, insulation, heat resistance are good, and cheap.2, silicates, phosphoric acid salt etc.3 other mineral powder are as mica powder, kaolin etc.4, the surface film of chemical method generation or the surface oxidation of generation.
Adopt above-mentioned megohmite insulant that amorphous powdered alloy is insulated, the megohmite insulant percentage by weight should be between the 0.2wt%-7wt% of mixture total weight amount.If megohmite insulant is very few, amorphous powdered alloy is difficult to obtain isolating more fully, contacts more; Perhaps insulating barrier is too thin, the easy breakdown insulating effect that loses under the electromagnetic induction effect, thus the magnetic core loss is big, and the high frequency magnetic permeability is low.If insulation divides too much, the interval between the powder is excessive, and magnetic core magnetic permeability reduces.The preferred weight percentage ranges of megohmite insulant is that 0.5wt% is to 5wt%.
The amorphous powdered alloy processability is relatively poor, especially aerosolization powder, difficult forming, the preferred following kind adhesive substance of the present invention is as adhesives: 1, organic bonding agent, as epoxylite, epoxylite generally uses as adhesives is at present industrial, and especially adhesive effect is better after mixing use with curing agent.2, inorganic adhesive, as phosphoric acid salt etc., the advantage of inorganic adhesive is that thermal endurance is good, and itself has good insulation property, and insulation and bonding double action are arranged, its amount can suitably increase, thereby can sufficient bonding powder.
Adopt above-mentioned adhesives, its bonding dosage accounts for mixture percentage and is no more than 5%.If bonding dosage is too much, the magnetic core performance descends, and magnetic permeability reduces.
The mixing of greasing substance its role is to: 1, make powder the time be easy to flow, thereby improve magnetic core density in compacting, 2, magnet ring and compacting tool set be difficult for taking place bonding, thereby be easy to the demoulding.The preferred stearate profit of the present invention, talcum powder etc. are as greasing substance, and its weight should be not more than the 2wt% of mixture weight.If lubricant is too much, can cause amorphous powdered alloy density decline in the magnetic core, thereby the magnetic core performance worsens, magnetic permeability reduces.
Mix fully in order to obtain insulating, the densification of powder core, the amorphous magnetic core that has excellent magnetic characteristics, the total amount of the preferred megohmite insulant of the present invention, adhesive substance and lubricant accounts for the 0.5wt% of mixture total weight amount to 10wt%; More preferably percentage by weight is that 1wt is to 7wt%.
Step 2
The preferred 500MPa-3000MPa of amorphous powdered alloy briquetting pressure of the present invention.Pressure is less than 500MPa, and powder is difficult to moulding, or has crackle to exist after the moulding, and magnetic permeability is low, and the magnetic core performance is not good.Pressure is greater than 3000MPa, and it is big that mould bears pressure, damage easily, and powder insulation difficulty, powder core loss height, quality factor are not good, and are therefore bad.Magnetic core briquetting pressure more preferably 800MPa to 2500Mpa.
Step 3
Amorphous powdered alloy cooling rate in preparation process is very fast, and unavoidably there is stress in inside; The magnetic core is subjected to the squeezing action of stirring action, press in preparation process, magnetic in-core portion also exists stress, the performance of these stress influence magnetic cores.By amorphous magnetic core is carried out annealing in process, can reach the purpose of eliminating powder internal stress, magnetic in-core portion's stress and improving magnetic property.Amorphous magnetic core annealing in process temperature should satisfy following condition: 1, annealing temperature should be carried out below the amorphous crystallization temperature.Because magnetic property worsens rapidly after the amorphous powdered alloy crystallization, show as that magnetic permeability reduces rapidly, loss increases.2, annealing temperature should not be lower than (T x-100 ℃), T wherein xBe the amorphous crystallization temperature.3, the preferred (T of powder annealing temperature x-70 ℃) to (T x-20 ℃) between.Because powder core annealing temperature is low excessively, thermal agitation is less, the amorphous core internal stress is difficult to fully be eliminated, and magnetic property is difficult to fully be promoted.The amorphous core annealing time should satisfy following condition: 1, powder core annealing time should be less than 3 hours.Because annealing time is long, efficient is low, increases manufacturing cost.2, powder core annealing time should because annealing time is too short, be difficult to reach the purpose of uniform treatment greater than 5 minutes during batch process, and the powder core performance is difficult to homogeneous.3, between preferred 30 minutes to 90 minutes of the powder core annealing time.Above-mentioned annealing process, the present invention preferably carries out under protective atmosphere, and protective atmosphere can be vacuum state, hydrogen state, nitrogen state or argon gas state.
Accompanying drawing 2 is the amorphous powdered alloy X ray diffracting spectrum of the embodiment of the invention 1 preparation.
Accompanying drawing 3 is the amorphous powdered alloy DSC curve of the embodiment of the invention 1 preparation.
Accompanying drawing 4 is static hysteresis loop under the 2000A/m for the magnetic core of the embodiment of the invention 1 preparation at maximum field.
Accompanying drawing 5 is the change curve of the amorphous magnetic core magnetic permeability of the embodiment of the invention 1 preparation with frequency.
Accompanying drawing 6 is the amorphous magnetic core of the embodiment of the invention 1 preparation and the MPP magnetic core quality factor of the comparing change curve with frequency.
Accompanying drawing 7 be under the amorphous magnetic core 100kHz of the embodiment of the invention 5 preparation magnetic permeability with the change curve of annealing temperature.
Accompanying drawing 8 be under the amorphous magnetic core 100kHz of the embodiment of the invention 5 preparation and the 1MHz quality factor with the change curve of annealing temperature.
Be the pairing coercive force H of static hysteresis loop under the 2000A/m for the amorphous magnetic core of the embodiment of the invention 5 preparation at maximum field among Fig. 9 cChange curve with annealing temperature.
Specific embodiments
Embodiment 1
Present embodiment adopts the Fe of water atomization method preparation 69Ni 5Al 4Sn 2P 10C 2B 4Si 4(the composition sequence number is 1) amorphous powdered alloy, raw material selection Fe, Ni, Al, Sn, P-Fe alloy, B-Fe alloy, graphite and Si.
The pattern photo of powder is seen Fig. 1.As seen from the figure, small particle powder is spherical substantially, and the bulky grain powder is that ellipsoid is capable, and small quantities of powder is an irregular powder.
Powder x-ray diffraction the results are shown in Figure 2.As seen from the figure, there is tangible wide collection of illustrative plates in X-ray diffraction, and does not have significant crystallization peak to exist, and illustrates that alloy powder is an amorphous structure, so Fe 72Ni 2Al 4Sn 2P 10C 2B 4Si 4Series can prepare amorphous powdered alloy by the water atomization method.
Fe 72Ni 2Al 4Sn 2P 10C 2B 4Si 4Powder DSC curve is seen Fig. 3.The programming rate that adopts when DSC measures is 10K/ minute.As seen from the figure, alloy glass transformation temperature T gBe 646K, crystallization temperature T xBe 695K.Its fusing point of high temperature dsc measurement T mBe 1209K, thereby can obtain the supercool liquid phase region Δ T of this alloy xBe 49K, reduction glass transformation temperature T RgBe 0.54.
Oxygen content in power the analysis showed that oxygen content in power is 3500ppm, illustrates that alloy has stronger antioxygenic property, and oxygen content is lower.
Screening obtains-300 purpose amorphous powdered alloys, at 440 ℃ of isothermal annealing 30min, adopts nitrogen protection in the annealing process.SiO with amorphous powdered alloy and 1.5wt% 2Powder, 1wt% epoxy resin, 0.3wt% zinc stearate evenly mix and oven dry, adopt alcohol as cosolvent during mixing.Adopt the pressure forming magnetic core of 2Gpa.The annealing of magnetic core is carried out under vacuum state, and annealing temperature is 400 ℃, and annealing time is 90 minutes.Adopt epoxy resin and polyester mixture that the magnetic wicking surface is sprayed, coating layer thickness is 100um.
Above-mentioned magnetic core be that static hysteresis loop under the 2000A/m provides in Fig. 4 at maximum field.As seen from the figure, magnetic core basic permanent permeance, its coercive force H of keeping in the test magnetic field range cBe 45A/m.
Provided the permeability measurement result of above-mentioned magnetic core magnetic property among Fig. 5.As seen from the figure, this magnetic core magnetic permeability is 46.9, and along with the variation magnetic core of frequency is keeping excellent permanent permeance, in the 5MHz scope, magnetic permeability drops to 46.4 by 46.9 at 6.3k, and the percentage of decline is less than 2%.
Provided of the variation of these magnetic core quality factor among Fig. 6, provided the comparing result of FeNiMo magnetic core as a comparison with frequency.As seen from the figure, amorphous alloy magnetic core has higher quality factor at high-frequency region.
Embodiment 2
Present embodiment adopts the Fe-Ni-Sn-Al-P-C-B-Si series non-crystaline amorphous metal step 4 of water atomization method preparation
For reaching the erosion that protection magnetic core is avoided the dry linting phenomenon occurring and is subjected to air etc., cause magnetic property to worsen, need be to the protection of spraying paint of magnetic core, the epoxy resin that the material preferred consolidation of spraying paint stress ratio is less or epoxy resin and polyester mixture.The preferred 50 μ m of coating thickness are to 300 μ m.
Step 5
Following method is adopted in the detection of each parameter of amorphous magnetic core performance of the present invention respectively: 1, the detection method of inductance and quality factor q, and adopting diameter is the copper enamelled wire of 0.2mm, uniform winding 10 circles are measured with the accurate electric impedance analyzer of Agilent 4294A; The magnetic permeability through type of magnetic core
μ e = l - L 0.4 π N 2 A · 10 8 Calculate, wherein l (is unit with cm) is the average length of magnetic path, and N is a coil turn, and A is that the magnetic circuit area is (with cm 2Be unit).2, the measurement of magnetic core static hysteresis loop adopts the simulation ballistic method to measure, and maximum field is 2000A/m.
Adopt alloy powder of the present invention, the magnetic core of using method for preparing has good soft magnet performance under high frequency.Particularly, amorphous magnetic core performance satisfies: under the frequency of 500kHz, quality factor is greater than 50, and magnetic permeability is greater than 40; Under the frequency of 1MHz, quality factor are greater than 30, and magnetic permeability is greater than 40; Under the frequency of 3MHz, magnetic core quality factor are greater than 20, and magnetic permeability is greater than 40; In the 1M scope, magnetic permeability descends less than 10% magnetic permeability at 100K.
Non-crystaline amorphous metal according to technical scheme preparation of the present invention has high amorphous formation ability and good antioxygenic property.This alloy has characteristics such as amorphous formation ability is strong, antioxygenic property good, soft magnet performance is superior concurrently, the amorphous powdered alloy that can prepare low oxygen content by atomization method obtains having high-gradient magnetism energy, low oxygen content, amorphous powdered alloy and corresponding magnetic ring thereof cheaply.
Description of drawings
Accompanying drawing 1 is the pattern photo of the amorphous powdered alloy of the embodiment of the invention 1 preparation.
Powder, raw material selection
Fe, Ni, Sn, Al, P-Fe alloy, graphite, B-Fe alloy and Si.
The concrete composition of present embodiment sees Table 1, and the glass transformation temperature of corresponding alloy, crystallization temperature, fusing point, reduction glass transformation temperature, supercool liquid phase region width are also listed in table 1 respectively. By table as seen, this series alloy, except composition 10 occurs the crystallization, other composition alloys all have high reduction glass transformation temperature, and minimum is 0.54, is 0.58 to the maximum, and alloy supercool liquid phase region width is greater than 20K.
Table 1
Sequence number Alloy atom forms   T g/K   T x/K   T m/K   T g/T m   (T x-T g)/K
  2   Fe 68.5Ni 3Al 7P 11.5C 3B 5   650   700   1209   0.54   50
  3   Fe 67Ni 7Sn 2Al 4P 10B 4C 2Si 4   654   694   1208   0.54   40
  4   Fe 70.5Ni 10Sn 1Al 4P 13C 2B 3Si 6   665   690   1204   0.55   25
  5   Fe 71Ni 4Sn 4Al 1P 10C 4B 2Si 4   666   698   1206   0.55   32
  6   Fe 72Ni 2Sn 1Al 3P 9C 2B 8Si 3   675   703   1211   0.56   28
  7   Fe 73Ni 1Sn 2Al 4P 10C 2B 4Si 4   668   715   1202   0.56   47
  8   Fe 73.5Ni 2Sn 5P 9.5C 2B 5Si 3   680   702   1200   0.57   22
  9   Fe 74.5Ni 1Sn 2xAl 2P 11.5B 4Si 5   698   729   1210   0.58   31
  10   Fe 77Ni 3Sn 1Al 3P 8C 2B 2Si 4   -   -   1208   -   -
Contrast 1   Fe 68.5Ni 3Al 7P 11.5C 3B 3Si 2   652   700   1209   0.54   48
The amorphous powdered alloy of mentioned component, oxygen content and the apparent density of its negative 300 amorphous powdered alloys provide in table 2. By table as seen, this series alloy is except contrast 1, and apparent density is 2.5g/cm3More than, oxygen content is below the 3900ppm, illustrates that alloy has stronger antioxygenic property.
The amorphous powdered alloy of mentioned component sieved obtain-300 purpose amorphous powdered alloys, at 440 ℃ of isothermal annealing 30min, adopt vacuum protection in the annealing process. SiO with amorphous powdered alloy and 1wt%2Powder, 1.5wt% epoxy resin, 0.3wt% zinc stearate evenly mix and oven dry, adopt alcohol as cosolvent during mixing. Adopt the pressure forming powder core of 2Gpa. Powder core annealing is carried out under vacuum state, and annealing temperature is 440 ℃, and annealing time is 60 minutes. Adopt epoxy resin and polyester mixture that the powder core surface is sprayed, coating layer thickness is 100um.
Adopt the amorphous alloy powder core of said method preparation, its performance provides in table 2, wherein contrasts 1 for atomization method is improper, the amorphous powdered alloy with elevated oxygen level, low-apparent-density that obtains. By as seen from Table 2, to compare with contrast 1, the alloy magnetic powder core that oxygen content in power is low, apparent density is larger has better performance, is embodied in that coercivity is low, magnetic conductivity is high; Composition 10, because crystallization has occured, magnetic property worsens; The alloy of other compositions (except 10, contrast 1) coercivity is less than 60A/m, and magnetic conductivity is all greater than 35, than under the magnetic conductivity 100kHz greater than 98%, under the 1MHz greater than quality factor under 90%, the 1MHz greater than 40.
Table 2
Sequence number Oxygen content (ppm) Apparent density (g/cm3) Structure   H c   (A/m)   μ   10kHz   μ   100kHz   μ 1MHz     Q 10kHz     Q 100kHz     Q 1MHz  
  2   3500   2.6 Amorphous   53   43   43   41   6   32   72
  3   2600   2.7 Amorphous   40   60   60   59   8   35   77
  4   3800   2.5 Amorphous   40   53   53   53   5   29   66
  5   3000   2.7 Amorphous   26   42   42   42   6   33   75
  6   3300   2.6 Amorphous   34   39   39   39   4.5   30   69
  7   2800   2.6 Amorphous   35   62   62   60   5.5   32   75
  8   3900   2.5 Amorphous   50   38   38   38   4   27   48
  9   3500   2.6 Amorphous   47   46   46   44   4.5   28   63
  10   3200   2.8 Crystallization   120   8   8   8   5   7   33
Contrast 1   5200   2.3 Amorphous   65   35   35   35   4.5   27   60
Embodiment 3
Present embodiment adopts the Fe-Co-Cr-Sn-Al-P-C-B-Si Amorphous Alloy powder of water atomization method preparation, raw material selection Fe, Co, Cr, Sn, Al, P-Fe alloy, graphite, B-Fe alloy and Si.
The concrete composition of present embodiment sees Table 3, and the glass transformation temperature of corresponding alloy, crystallization temperature, fusing point, reduction glass transformation temperature, supercool liquid phase region width are also listed in table 3 respectively. By table as seen, this series alloy, except composition 20 can not form whole amorphous, other composition alloys all had high reduction glass transformation temperature, and minimum is 0.58, is 0.60 to the maximum, and alloy has supercool liquid phase region width greater than 20K.
Table 3
Sequence number Alloy atom forms   T g/K   T x/K   T m/K   T g/T m   (T x-T g)/K
  11   Fe 70Co 2Cr 2Sn 2Al 4P 10C 2B 4Si 4   705   744   1208   0.58   39
  12   Fe 68.5Co 2Cr 1Sn 2Al 7P 11.5C 3B 3Si 2   715   740   1197   0.60   25
  13   Fe 68.5Co 1Cr 5Sn 3Al 2P 11.5C 5B 2Si 2   715   753   1223   0.58   38
  14   Fe 69.5Co 1Cr 0.5Sn 1Al 4P 13C 2B 3Si 6   701   738   1183   0.59   37
  15   Fe 69.5Co 2Cr 4Sn 4Al 1P 10C 4B 2Si 4   723   758   1215   0.60   35
  16   Fe 70Co 2Cr 2Sn 1Al 3P 9C 2B 8Si 3   704   739   1216   0.58   35
  17   Fe 71Co 2Cr 1Sn 2Al 4P 10C 2B 4Si 4   671   724   1204   0.56   53
  18   Fe 71.5Co 5Cr 1Al 2P 10.5C 2B 5Si 3   698   731   1201   0.58   33
  19   Fe 72.5Co 2Cr 2Al 4P 9.5C 1B 4Si 5   701   732   1209   0.58   31
  20   Fe 75Co 3Cr 3Al 3P 8C 2B 2Si 4   -   -   1250   -   -
The amorphous powdered alloy of mentioned component, oxygen content and the apparent density of its negative 300 amorphous powdered alloys provide in table 4. By table as seen, this series alloy apparent density all is not less than 2.5g/cm3, oxygen content illustrates that all less than 3300ppm alloy has stronger antioxygenic property.
The amorphous powdered alloy of mentioned component sieved obtain-300 purpose amorphous powdered alloys, at 440 ℃ of isothermal annealing 30min, adopt vacuum protection in the annealing process. SiO with amorphous powdered alloy and 1wt%2Powder, 1.5wt% epoxy resin, 0.3wt% zinc stearate evenly mix and oven dry, adopt alcohol as cosolvent during mixing. Adopt the pressure forming powder core of 2Gpa. Powder core annealing is carried out under vacuum state, and annealing temperature is 440 ℃, and annealing time is 60 minutes. Adopt epoxy resin and polyester mixture that the powder core surface is sprayed, coating layer thickness is 100um.
Adopt the amorphous alloy powder core of said method preparation, its performance provides in table 4, by table 4 as seen, except crystallization occurs in composition 20, the powder core mis-behave, all the other compositions all have better magnetic property, and magnetic conductivity is not less than 45.
The alloy of other compositions (except 10, contrast 1) coercivity is less than 60A/m, magnetic conductivity all greater than 35,1 than under the magnetic conductivity 00kHz greater than 98%, under the 1MHz greater than quality factor under 90%, the 1MHz greater than 60.
Table 4
Sequence number Oxygen content (ppm) Apparent density (g/cm3) Structure   H c   (A/m)   μ   10kHz   μ   100kHz   μ   1MHz   Q 10kHz     Q 100kHz     Q 1MHz  
  11   2600   2.8.0 Amorphous   46   48   48   47   7   34   72
  12   2900   2.9 Amorphous   37   60   60   58   8   38   85
  13   2500   2.8 Amorphous   40   65   65   64   7   35   80
  14   3000   2.8 Amorphous   41   65   65   64   6   33   75
  15   2700   2.6 Amorphous   49   60   60   59   6   30   72
  16   2800   2.6 Amorphous   50   53   53   52   6   32   75
  17   3300   2.5 Amorphous   47   49   49   48   5   27   64
  18   3000   2.7 Amorphous   54   45   45   44   4.5   28   68
  19   3200   2.7 Amorphous   52   46   46   45   4.5   28   67
  20   2800   2.7 Crystallization   118   12   12   12   5   7   34
Embodiment 4
Present embodiment adopts antivacuum aerosolization method to prepare Fe-Co-Ni-Cr-Sn-Al-P-C-B-Si Amorphous Alloy powder, raw material selection Fe, Co, Ni, Cr, Sn, Al, P-Fe alloy, graphite, B-Fe alloy and Si.
The concrete composition of present embodiment sees Table 5, and the glass transformation temperature of corresponding alloy, crystallization temperature, fusing point, reduction glass transformation temperature, supercool liquid phase region width are also listed in table 5 respectively.By table as seen, this series alloy, except that composition 25 can not form whole amorphous, other composition alloys all had high reduction glass transformation temperature, and minimum is 0.58, is 0.60 to the maximum, and alloy has supercool liquid phase region width greater than 20K.
Table 5
Sequence number Alloy atom is formed T g/K T x/K T m/K T g/T m (T x-T g)/K
21 Fe 71Co 2Sn 2Al 4P 10C 2B 5Si 4 703 740 1208 0.58 37
22 Fe 71Ni 2Cr 1Al 4P 11C 2B 6Si 2 715 745 1197 0.60 30
23 Fe 72.5Co 1Ni 1Sn 3Al 2P 11.5C 5B 2Si 2 708 746 1223 0.58 38
24 Fe 63Ni 3Co 3Cr 0.5Al 4P 13C 2B 3Si 6 720 743 1183 0.61 23
25 Fe 63Ni 5Co 3Cr 2Sn 4Al 1P 10C 4B 2Si 4 - - 1215 - -
The amorphous powdered alloy of mentioned component, the oxygen content and the apparent density of its negative 350 amorphous powdered alloys provide in table 6.By table as seen, this series alloy apparent density all is not less than 3.6g/cm 3, oxygen content is all less than 2000ppm.
The amorphous powdered alloy of mentioned component sieved obtain-350 purpose amorphous powdered alloys,, adopt vacuum protection in the annealing process at 400 ℃ of isothermal annealing 30min.SiO with amorphous powdered alloy and 1wt% 2Powder, 2wt% epoxy resin, 0.3wt% zinc stearate evenly mix and oven dry, adopt alcohol as cosolvent during mixing.Adopt the pressure forming magnetic core of 2.4Gpa.The annealing of magnetic core is carried out under vacuum state, and annealing temperature is 440 ℃, and annealing time is 60 minutes.Adopt epoxy resin and polyester mixture that the magnetic wicking surface is sprayed, coating layer thickness is 100um.
Adopt the amorphous alloy magnetic core of method for preparing, its performance provides in table 6, by table 6 as seen, remove composition 25 crystallization takes place, the magnetic core performance worsens, and the alloy coercive force of other compositions is less than 40A/m, and magnetic permeability is all greater than 60, than under the magnetic permeability 100kHz greater than 98%, under the 1MHz greater than 90%, quality factor are greater than 60 under the 1MHz.
Table 6
Sequence number Oxygen content (ppm) Apparent density (g/cm 3) Structure H c (A/m) μ 10kHz μ 100kHz μ 1MHz Q 10kHz Q 00kHz Q 1MHz
21 1500 3.6 Amorphous 32 72 72 70 9 45 98
22 1200 3.7 Amorphous 28 70 70 68 9 40 88
23 1250 3.7 Amorphous 26 68 68 66 9 40 92
24 1100 3.7 Amorphous 25 75 75 73 9 41 96
25 800 3.7 Crystallization 68 13 13 13 6 9 42
Embodiment 5
Adopt the method identical with embodiment 1 to prepare amorphous powdered alloy, the magnetic core prepares in each step also identical, and different is to have changed heat treatment temperature.
Provided under the magnetic core 100kHz magnetic permeability among Fig. 7 with the change curve of annealing temperature.As seen from the figure, this magnetic core magnetic permeability raises along with the rising of heat treatment temperature, reaches maximum at 440 ℃ of annexes, and the back reduces along with the rising of annealing temperature, and maximum permeability is about 50.
Quality factor have been provided under magnetic core 100kHz and the 1MHz among Fig. 8 with the change curve of annealing temperature, its Changing Pattern and magnetic permeability Changing Pattern are similar, difference is that it is 380 ℃ of annexes that the maximum quality factor of magnetic core appear at annealing temperature, and maximum quality factor are about 75 during 100kHz; Be about 35 during 1MHz.
Having provided maximum field among Fig. 9 is the pairing coercive force H of 2000A/m magnetic core static hysteresis loop cChange curve with annealing temperature.As seen from the figure, the variation tendency of coercitive variation tendency and magnetic core magnetic permeability is opposite fully, and minimum coercive force is about 44A/m.

Claims (18)

1, a kind of amorphous powdered alloy with good high-frequency soft magnetic performance is characterized in that, its alloying component atomic percent composition satisfies relational expression: (Fe 1-xM x) 100-a-b-cP aT bD c
Wherein, M is at least a among Co, the Ni; T be among Al, C, B, the Si more than three kinds; D is at least a among Sn, Cr, Mn, Mo, W, V, Nb, Ta, Ti, Zr, Hf, Pt, Pd, the Au; X is 0.01-0.16; A is 8-15; B is 10-25; C is 0.5-6.
According to the described amorphous powdered alloy of claim 1, it is characterized in that 2, x is 0.01-0.12; A is 9-12; B is 10-23; C is 1-5.
3, according to the described amorphous powdered alloy of claim 1, it is characterized in that 22≤(a+b+c)≤38.
4. according to the described amorphous powdered alloy of claim 1, it is characterized in that, reduction glass transformation temperature Trg 〉=0.53 of this amorphous powdered alloy, Trg=Tg/Tm wherein, Tg is a glass transformation temperature, Tm is an alloy melting point.
5. according to the described amorphous powdered alloy of claim 1, it is characterized in that, the supercool liquid phase region Δ Tx 〉=20K of this amorphous powdered alloy, Δ Tx=Tx-Tg wherein, Tx is a crystallization temperature.
6. according to the described amorphous powdered alloy of claim 1, it is characterized in that the oxygen content in power of this amorphous powdered alloy is below 4000ppm.
7. preparation method with amorphous powdered alloy of good high-frequency soft magnetic performance, it is characterized in that: the alloy that adopts one of any composition of claim 1-3, adopt atomizing type to prepare alloy powder, described atomizing type is water atomization and/or aerosolization, and described aerosol turns to vacuum aerosolization, antivacuum aerosolization, regulate one or more or its combination in the aerosolization.
8. according to the preparation method of the described amorphous powdered alloy of claim 7, it is characterized in that apparent density of powder ρ satisfies: ρ 〉=2.4g/cm 3
9. non-crystaline amorphous metal powder magnetic core with good high-frequency soft magnetic performance, it is characterized in that, comprise following components in weight percentage: insulating compound 0.2%-7%, bonding agent 0.01-5%, lubricant 0.01-2%, all the other are any one described non-crystaline amorphous metal powder of claim 1-6.
10. non-crystaline amorphous metal powder magnetic core according to claim 9 is characterized in that, described insulating compound is selected from following at least a or its combination of respectively organizing in the material:
Be selected from SiO 2, Cao, Al 2O 3, TiO 2Oxide powder;
Be selected from the salt of silicates, phosphoric acid salt;
Be selected from mica powder, kaolinic mineral powder; With
The surface film that chemical method generates or the surface oxidation of generation.
11. non-crystaline amorphous metal powder magnetic core according to claim 9, it is characterized in that, described bonding agent is organic bonding agent and/or inorganic adhesive, wherein: the organic bonding agent be selected from epoxylite, at least a in the epoxylite, inorganic adhesive is selected from least a in the phosphoric acid salt.
12. non-crystaline amorphous metal powder magnetic core according to claim 9 is characterized in that, described lubricant is selected from the stearate profit, talcum powder is at least a or its combination.
13. non-crystaline amorphous metal powder magnetic core according to claim 9 is characterized in that, its magnetic property satisfy following at least one, several or its combination:
Magnetic permeability is more than 35;
Quality factor q is not less than 30 under 1MHz;
Under 100kHz, be not less than 98% than magnetic permeability, under 1MHz, be not less than 90%;
Maximum field is the pairing coercive force H of the static hysteresis loop of 2000A/m cBelow 70A/m.
14. the preparation method with non-crystaline amorphous metal powder magnetic core of good high-frequency soft magnetic performance is characterized in that this method may further comprise the steps:
(a), adopt insulating compound, bonding agent and the mix lubricant of claim any one described amorphous powdered alloy of 1-6 and desired content and be dried to dry powder;
(b), above-mentioned dried powder is pressed in makes the magnetic core under the 500MPa-3000MPa pressure;
(c), the magnetic core with press forming carries out annealing in process below the amorphous crystallization temperature.
15. the preparation method of non-crystaline amorphous metal powder magnetic core according to claim 14 is characterized in that, after described step (c), further may further comprise the steps: (d), the processing of spraying paint of magnetic core; (e), the magnetic core performance detects.
16. the preparation method of non-crystaline amorphous metal powder magnetic core according to claim 14 is characterized in that, in the described step (c), described magnetic core annealing in process temperature is at (T x-100 ℃) to T xBetween, T xBe the amorphous crystallization temperature; Be annealed into 5 minutes to 300 minutes; Atmosphere is a kind of in vacuum, nitrogen, the argon gas atmosphere.
17. the preparation method according to claim 14,16 described non-crystaline amorphous metal powder magnetic cores is characterized in that in the described step (c), annealing temperature is at (T x-70 ℃) to (T x-20 ℃) between, T xBe the amorphous crystallization temperature.
18. the preparation method of non-crystaline amorphous metal powder magnetic core according to claim 14 is characterized in that, the magnetic property of the magnetic core that obtains satisfies following at least one or its combination:
Magnetic permeability is more than 35;
Quality factor q is not less than 30 under 1MHz;
Under 100kHz, be not less than 98% than magnetic permeability, under 1MHz, be not less than 90%;
Maximum field is the pairing coercive force H of the static hysteresis loop of 2000A/m cBelow 70A/m.
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EP1933337B8 (en) * 2006-12-15 2010-09-01 Alps Green Devices Co., Ltd Fe-based amorphous magnetic alloy and magnetic sheet
WO2009037824A1 (en) * 2007-09-18 2009-03-26 Nec Tokin Corporation Soft magnetic amorphous alloy
CN102264938B (en) 2009-01-23 2013-05-15 阿尔卑斯绿色器件株式会社 Iron-based soft magnetic alloy and dust core comprising the iron-based soft magnetic alloy
US9328404B2 (en) * 2009-04-20 2016-05-03 Lawrence Livermore National Security, Llc Iron-based amorphous alloys and methods of synthesizing iron-based amorphous alloys
EP2463396B1 (en) 2009-08-07 2019-04-03 Alps Alpine Co., Ltd. Fe-based amorphous alloy, dust core formed using the fe-based amorphous alloy, and dust core with embedded coil
WO2011075516A2 (en) 2009-12-18 2011-06-23 President And Fellows Of Harvard College Active scaffolds for on-demand drug and cell delivery
TWI441929B (en) 2011-01-17 2014-06-21 Alps Green Devices Co Ltd Fe-based amorphous alloy powder, and a powder core portion using the Fe-based amorphous alloy, and a powder core
KR101385756B1 (en) * 2013-01-24 2014-04-21 주식회사 아모그린텍 Manufacturing methods of fe-based amorphous metallic powders and soft magnetic cores
DE102013101364B4 (en) * 2013-02-12 2023-02-02 Tdk Electronics Ag Electrical transformer component
JP6260086B2 (en) * 2013-03-04 2018-01-17 新東工業株式会社 Iron-based metallic glass alloy powder
US10363548B2 (en) 2016-01-22 2019-07-30 University Of North Texas Aluminum based metallic glass powder for efficient degradation of AZO dye and other toxic organic chemicals
US20190013129A1 (en) * 2017-07-06 2019-01-10 Panasonic Intellectual Property Management Co., Ltd. Dust core
KR101821760B1 (en) 2017-11-09 2018-01-29 (주)한국코팅 Fe-Cr-Ni-B Based on the Wire for the Arc Thermal Spray with Ultra High Hardness Property
CN108793756B (en) * 2018-06-22 2021-12-03 贵州佰博新材料科技有限公司 Glass powder for insulating and coating iron-silicon-aluminum magnetic powder core and preparation method thereof
JP2022157035A (en) * 2021-03-31 2022-10-14 Tdk株式会社 Soft magnetic alloy and magnetic component

Family Cites Families (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4152144A (en) * 1976-12-29 1979-05-01 Allied Chemical Corporation Metallic glasses having a combination of high permeability, low magnetostriction, low ac core loss and high thermal stability
US4187128A (en) * 1978-09-26 1980-02-05 Bell Telephone Laboratories, Incorporated Magnetic devices including amorphous alloys
US4217135A (en) * 1979-05-04 1980-08-12 General Electric Company Iron-boron-silicon ternary amorphous alloys
US4495487A (en) * 1981-11-02 1985-01-22 Allied Corporation Amorphous antipilferage marker
JPS58213857A (en) * 1982-06-04 1983-12-12 Takeshi Masumoto Amorphous iron alloy having superior fatigue characteristic
US4881989A (en) * 1986-12-15 1989-11-21 Hitachi Metals, Ltd. Fe-base soft magnetic alloy and method of producing same
JP2611994B2 (en) * 1987-07-23 1997-05-21 日立金属株式会社 Fe-based alloy powder and method for producing the same
JP3904250B2 (en) * 1995-06-02 2007-04-11 独立行政法人科学技術振興機構 Fe-based metallic glass alloy
JPH09256122A (en) * 1996-03-19 1997-09-30 Unitika Ltd Ferrous amorphous alloy
JP3710226B2 (en) * 1996-03-25 2005-10-26 明久 井上 Quench ribbon made of Fe-based soft magnetic metallic glass alloy
US6053989A (en) * 1997-02-27 2000-04-25 Fmc Corporation Amorphous and amorphous/microcrystalline metal alloys and methods for their production
US6011475A (en) * 1997-11-12 2000-01-04 Vacuumschmelze Gmbh Method of annealing amorphous ribbons and marker for electronic article surveillance
US6594157B2 (en) * 2000-03-21 2003-07-15 Alps Electric Co., Ltd. Low-loss magnetic powder core, and switching power supply, active filter, filter, and amplifying device using the same
JP3771224B2 (en) * 2002-09-11 2006-04-26 アルプス電気株式会社 Amorphous soft magnetic alloy powder and powder core and radio wave absorber using the same
WO2005020252A1 (en) * 2003-08-22 2005-03-03 Nec Tokin Corporation Magnetic core for high frequency and inductive component using same
JP4562022B2 (en) * 2004-04-22 2010-10-13 アルプス・グリーンデバイス株式会社 Amorphous soft magnetic alloy powder and powder core and electromagnetic wave absorber using the same

Cited By (26)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103794327A (en) * 2006-02-02 2014-05-14 Nec东金株式会社 Amorphous soft magnetic alloy and inductance component using the same
US10984932B2 (en) 2006-02-02 2021-04-20 Tokin Corporation Amorphous soft magnetic alloy and inductance component using the same
CN101641455B (en) * 2007-03-22 2012-05-30 日立金属株式会社 Soft magnetic ribbon, magnetic core, magnetic part and process for producing soft magnetic ribbon
WO2009067861A1 (en) * 2007-11-27 2009-06-04 Advanced Technology & Materials Co., Ltd Fe-based amorphous soft magnetic alloy powder, magnetic powder core comprising the powder and manufacturing method of the same
CN101492794B (en) * 2008-01-21 2014-06-25 安泰科技股份有限公司 Iron based amorphous alloy material and uses thereof
CN105355356A (en) * 2009-12-25 2016-02-24 株式会社田村制作所 Dust core and method for manufacturing the same
CN101935742A (en) * 2010-09-21 2011-01-05 中国矿业大学 Annealing method for preparing nanocrystalline alloy with excellent soft magnetic property
CN101935742B (en) * 2010-09-21 2013-01-02 中国矿业大学 Annealing method for preparing nanocrystalline alloy with excellent soft magnetic property
CN102543349A (en) * 2012-03-27 2012-07-04 广州有色金属研究院 Ferrum (Fe) - silicon (Si) - nickel (Ni) -aluminum (Al) - titanium (Ti) soft magnetic alloy powder
CN103219119A (en) * 2013-04-18 2013-07-24 安泰科技股份有限公司 Preparation method of mu90 high-permeability Fe-based amorphous magnetic powder core
CN105873697A (en) * 2013-12-20 2016-08-17 霍加纳斯股份有限公司 Soft magnetic powder mix
CN105873697B (en) * 2013-12-20 2019-05-10 霍加纳斯股份有限公司 Soft magnetic powder mixture
CN104036901A (en) * 2014-05-28 2014-09-10 浙江大学 High-permeability low-loss metal soft-magnetism composite material and preparing method thereof
CN104036901B (en) * 2014-05-28 2016-08-24 浙江大学 A kind of high magnetic conductivity and low loss soft magnetic metal composite and preparation method thereof
CN105063516A (en) * 2015-08-01 2015-11-18 江苏华源防爆电机有限公司 High-magnetic-permeability and low-loss amorphous material for engine
CN105624588A (en) * 2015-12-30 2016-06-01 安泰科技股份有限公司 Soft magnetic alloy for electromagnetic shielding and preparation method for soft magnetic alloy
CN107365950A (en) * 2017-07-24 2017-11-21 广东咏旺新材料科技有限公司 Fe Si B Nb Cu are Fe-based amorphous/nanocrystalline magnetically soft alloy material and preparation and Technology for Heating Processing
CN107365950B (en) * 2017-07-24 2019-03-19 广东咏旺新材料科技有限公司 Fe-Si-B-Nb-Cu is Fe-based amorphous/nanocrystalline magnetically soft alloy material and preparation and heat treatment process
CN108231393A (en) * 2017-12-13 2018-06-29 横店集团东磁股份有限公司 A kind of preparation method of high magnetic permeability iron nickel magnetic core
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